#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179139 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310080.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4310080
loop_
_publ_author_name
'Julien Massue'
'Nathalie Bellec'
'Stéphanie Chopin'
'Eric Levillain'
'Thierry Roisnel'
'Rodolphe Clérac'
'Dominique Lorcy'
_publ_section_title
;
Electroactive Ligands: The First Metal Complexes of
Tetrathiafulvenyl-Acetylacetonate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8740
_journal_page_last               8748
_journal_paper_doi               10.1021/ic051017r
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H40 N2 Ni1 O4 S16'
_chemical_formula_sum            'C38 H40 N2 Ni O4 S16'
_chemical_formula_weight         1160.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-11-15T12:35:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 107.370(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   19.953(5)
_cell_length_b                   9.397(5)
_cell_length_c                   28.325(5)
_cell_measurement_reflns_used    32148
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     5069(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (ALtomare, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.292526E-1
_diffrn_orient_matrix_UB_12      0.568957E-1
_diffrn_orient_matrix_UB_13      0.162845E-1
_diffrn_orient_matrix_UB_21      -0.425905E-1
_diffrn_orient_matrix_UB_22      -0.547906E-1
_diffrn_orient_matrix_UB_23      -0.187635E-1
_diffrn_orient_matrix_UB_31      0.93836E-2
_diffrn_orient_matrix_UB_32      -0.713173E-1
_diffrn_orient_matrix_UB_33      0.274069E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            30277
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.8848
_exptl_absorpt_correction_T_min  0.7093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0480P)²+4.7547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                4303
_reflns_number_total             5815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051017rsi20050622_054911.cif
_cod_data_source_block           acacni2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4310080
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.25 0.25 0.5 0.04149(13) Uani 1 2 d S . .
S1 S 0.03081(4) 0.37244(8) 0.54847(3) 0.05405(19) Uani 1 1 d . . .
S2 S -0.05464(4) 0.40938(9) 0.63121(3) 0.0693(2) Uani 1 1 d . . .
S3 S 0.07610(4) 0.08346(7) 0.59437(2) 0.05393(19) Uani 1 1 d . . .
S4 S -0.00748(4) 0.11266(8) 0.66405(3) 0.05608(19) Uani 1 1 d . . .
S5 S 0.16195(4) -0.18441(8) 0.66310(3) 0.0610(2) Uani 1 1 d . . .
S6 S 0.07672(4) -0.14178(8) 0.73001(3) 0.05550(19) Uani 1 1 d . . .
S7 S 0.26952(5) -0.36322(9) 0.73606(4) 0.0761(3) Uani 1 1 d . . .
S8 S 0.17212(5) -0.31793(9) 0.81154(3) 0.0710(2) Uani 1 1 d . . .
N1 N 0.27636(11) 0.4597(2) 0.48300(7) 0.0477(5) Uani 1 1 d . . .
O1 O 0.14773(9) 0.27910(19) 0.46341(6) 0.0466(4) Uani 1 1 d . . .
O2 O 0.23169(9) 0.3312(2) 0.56079(6) 0.0490(4) Uani 1 1 d . . .
C1 C 0.24127(16) 0.5237(3) 0.44100(10) 0.0594(7) Uani 1 1 d . . .
H1 H 0.205 0.4744 0.4187 0.071 Uiso 1 1 calc R . .
C2 C 0.2561(2) 0.6593(4) 0.42906(13) 0.0749(9) Uani 1 1 d . . .
H2 H 0.23 0.7008 0.3995 0.09 Uiso 1 1 calc R . .
C3 C 0.3096(2) 0.7322(4) 0.46111(15) 0.0800(10) Uani 1 1 d . . .
H3 H 0.3206 0.824 0.4537 0.096 Uiso 1 1 calc R . .
C4 C 0.34657(18) 0.6685(4) 0.50420(14) 0.0765(9) Uani 1 1 d . . .
H4 H 0.3836 0.7159 0.5266 0.092 Uiso 1 1 calc R . .
C5 C 0.32833(15) 0.5329(3) 0.51413(11) 0.0603(7) Uani 1 1 d . . .
H5 H 0.3533 0.4905 0.5438 0.072 Uiso 1 1 calc R . .
C6 C 0.17831(17) 0.4269(3) 0.61638(10) 0.0630(8) Uani 1 1 d . . .
H6A H 0.2267 0.4373 0.6353 0.095 Uiso 1 1 calc R . .
H6B H 0.155 0.3667 0.6339 0.095 Uiso 1 1 calc R . .
H6C H 0.1562 0.5187 0.6114 0.095 Uiso 1 1 calc R . .
C7 C 0.17367(14) 0.3611(3) 0.56695(9) 0.0441(6) Uani 1 1 d . . .
C8 C 0.10724(13) 0.3343(3) 0.53157(9) 0.0429(5) Uani 1 1 d . . .
C9 C 0.09812(13) 0.2904(3) 0.48205(9) 0.0418(5) Uani 1 1 d . . .
C10 C 0.02661(14) 0.2544(3) 0.44781(11) 0.0586(7) Uani 1 1 d . . .
H10A H 0.0307 0.2268 0.4162 0.088 Uiso 1 1 calc R . .
H10B H -0.0034 0.3362 0.4439 0.088 Uiso 1 1 calc R . .
H10C H 0.0069 0.1773 0.4615 0.088 Uiso 1 1 calc R . .
C11 C 0.0050(3) 0.4940(5) 0.68232(18) 0.136(2) Uani 1 1 d . . .
H11A H -0.0154 0.5805 0.6897 0.203 Uiso 1 1 calc R . .
H11B H 0.0476 0.5156 0.6746 0.203 Uiso 1 1 calc R . .
H11C H 0.0154 0.4319 0.7105 0.203 Uiso 1 1 calc R . .
C12 C -0.00563(13) 0.2591(3) 0.62583(9) 0.0477(6) Uani 1 1 d . . .
C13 C 0.03035(13) 0.2441(3) 0.59315(9) 0.0437(5) Uani 1 1 d . . .
C14 C 0.06011(14) 0.0216(3) 0.64873(9) 0.0457(6) Uani 1 1 d . . .
C15 C 0.09568(13) -0.0851(3) 0.67638(9) 0.0462(6) Uani 1 1 d . . .
C16 C 0.13107(18) -0.1964(4) 0.84289(10) 0.0765(9) Uani 1 1 d . . .
H16A H 0.1378 -0.229 0.8761 0.115 Uiso 1 1 calc R . .
H16B H 0.0817 -0.1913 0.8258 0.115 Uiso 1 1 calc R . .
H16C H 0.1517 -0.1038 0.8436 0.115 Uiso 1 1 calc R . .
C18 C 0.19374(14) -0.2591(3) 0.72272(10) 0.0517(6) Uani 1 1 d . . .
C17 C 0.15432(14) -0.2407(3) 0.75300(9) 0.0476(6) Uani 1 1 d . . .
C19 C 0.3351(2) -0.2324(5) 0.73896(19) 0.1159(16) Uani 1 1 d . . .
H19A H 0.3802 -0.2776 0.7463 0.174 Uiso 1 1 calc R . .
H19B H 0.3354 -0.1647 0.7644 0.174 Uiso 1 1 calc R . .
H19C H 0.325 -0.1844 0.7077 0.174 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 1 -6 0.04
-1 7 15 0.084
-1 0 13 0.073
-1 -5 12 0.054
-4 1 8 0.053
6 -1 -5 0.033
1 0 18 0.122
4 2 -3 0.044
-2 -1 5 0.048
-9 -4 -5 0.079
2 1 -6 0.077
-10 3 11 0.09
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.00(9) 7_556 . ?
O1 Ni1 O2 88.51(7) 7_556 7_556 ?
O1 Ni1 O2 91.49(7) . 7_556 ?
O1 Ni1 O2 91.49(7) 7_556 . ?
O1 Ni1 O2 88.51(7) . . ?
O2 Ni1 O2 180.00(4) 7_556 . ?
O1 Ni1 N1 87.78(8) 7_556 . ?
O1 Ni1 N1 92.22(8) . . ?
O2 Ni1 N1 92.12(8) 7_556 . ?
O2 Ni1 N1 87.88(8) . . ?
O1 Ni1 N1 92.22(8) 7_556 7_556 ?
O1 Ni1 N1 87.78(8) . 7_556 ?
O2 Ni1 N1 87.88(8) 7_556 7_556 ?
O2 Ni1 N1 92.12(8) . 7_556 ?
N1 Ni1 N1 180 . 7_556 ?
C13 S1 C8 104.32(11) . . ?
C12 S2 C11 100.22(17) . . ?
C13 S3 C14 94.12(12) . . ?
C14 S4 C12 94.02(12) . . ?
C15 S5 C18 94.89(12) . . ?
C15 S6 C17 95.02(12) . . ?
C18 S7 C19 101.54(18) . . ?
C17 S8 C16 102.29(14) . . ?
C1 N1 C5 117.1(3) . . ?
C1 N1 Ni1 121.38(19) . . ?
C5 N1 Ni1 121.54(19) . . ?
C9 O1 Ni1 126.83(15) . . ?
C7 O2 Ni1 127.96(16) . . ?
N1 C1 C2 123.1(3) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 122.9(3) . . ?
N1 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C7 C8 124.5(2) . . ?
O2 C7 C6 114.7(2) . . ?
C8 C7 C6 120.8(2) . . ?
C9 C8 C7 124.3(2) . . ?
C9 C8 S1 117.39(19) . . ?
C7 C8 S1 118.07(18) . . ?
O1 C9 C8 123.6(2) . . ?
O1 C9 C10 115.1(2) . . ?
C8 C9 C10 121.3(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
S2 C11 H11A 109.5 . . ?
S2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
S2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 S2 125.1(2) . . ?
C13 C12 S4 117.3(2) . . ?
S2 C12 S4 117.59(15) . . ?
C12 C13 S1 123.2(2) . . ?
C12 C13 S3 117.35(19) . . ?
S1 C13 S3 119.41(14) . . ?
C15 C14 S4 122.16(19) . . ?
C15 C14 S3 123.8(2) . . ?
S4 C14 S3 114.08(14) . . ?
C14 C15 S5 125.2(2) . . ?
C14 C15 S6 121.4(2) . . ?
S5 C15 S6 113.38(14) . . ?
S8 C16 H16A 109.5 . . ?
S8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C18 S7 124.8(2) . . ?
C17 C18 S5 116.8(2) . . ?
S7 C18 S5 118.13(16) . . ?
C18 C17 S8 124.3(2) . . ?
C18 C17 S6 116.9(2) . . ?
S8 C17 S6 118.61(15) . . ?
S7 C19 H19A 109.5 . . ?
S7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0125(17) 7_556 ?
Ni1 O1 2.0125(17) . ?
Ni1 O2 2.0139(16) 7_556 ?
Ni1 O2 2.0139(16) . ?
Ni1 N1 2.131(2) . ?
Ni1 N1 2.131(2) 7_556 ?
S1 C13 1.750(2) . ?
S1 C8 1.766(2) . ?
S2 C12 1.750(3) . ?
S2 C11 1.765(4) . ?
S3 C13 1.759(3) . ?
S3 C14 1.762(2) . ?
S4 C14 1.757(3) . ?
S4 C12 1.758(3) . ?
S5 C15 1.749(3) . ?
S5 C18 1.763(3) . ?
S6 C15 1.754(2) . ?
S6 C17 1.756(3) . ?
S7 C18 1.745(3) . ?
S7 C19 1.779(4) . ?
S8 C17 1.747(3) . ?
S8 C16 1.788(3) . ?
N1 C1 1.331(3) . ?
N1 C5 1.334(3) . ?
O1 C9 1.258(3) . ?
O2 C7 1.253(3) . ?
C1 C2 1.373(5) . ?
C1 H1 0.93 . ?
C2 C3 1.361(5) . ?
C2 H2 0.93 . ?
C3 C4 1.362(5) . ?
C3 H3 0.93 . ?
C4 C5 1.377(5) . ?
C4 H4 0.93 . ?
C5 H5 0.93 . ?
C6 C7 1.508(3) . ?
C6 H6A 0.96 . ?
C6 H6B 0.96 . ?
C6 H6C 0.96 . ?
C7 C8 1.425(4) . ?
C8 C9 1.421(3) . ?
C9 C10 1.505(4) . ?
C10 H10A 0.96 . ?
C10 H10B 0.96 . ?
C10 H10C 0.96 . ?
C11 H11A 0.96 . ?
C11 H11B 0.96 . ?
C11 H11C 0.96 . ?
C12 C13 1.338(4) . ?
C14 C15 1.339(3) . ?
C16 H16A 0.96 . ?
C16 H16B 0.96 . ?
C16 H16C 0.96 . ?
C18 C17 1.337(4) . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
